Screening of sulphonamides in egg using gas chromatography-mass-selective detection and liquid chromatography-mass spectrometry. 1999

J A Tarbin, and P Clarke, and G Shearer
Ministry of Agriculture, Fisheries and Food, Central Science Laboratory, Sand Hutton, York, UK.

A rapid extraction and clean-up procedure for sulphonamide antibiotics in eggs suitable for both GC-MSD and LC-MS end determinations has been developed. The drugs were extracted using acetonitrile, acidified using acetic acid and cleaned-up using cation- and anion-exchange. For determination by GC-MSD, extracts were derivatised with diazomethane followed by pentafluoropropionic acid anhydride. For LC-MS extracts were taken up in water and used directly. The methodology developed was validated at the 100 and 25 microg kg(-1) levels, equivalent to the MRL and one quarter of the MRL. Results for the GC-MS procedure were quantitated against deuterated sulphadiazine with relative recoveries ranging from 54% for sulphachloropyridazine to 135.5% for sulphamethazine. Recoveries for the LC-MS procedure ranged from 33% for sulphaguanidine to 92% for sulphamethazine and sulphadimethoxine.

UI MeSH Term Description Entries
D008401 Gas Chromatography-Mass Spectrometry A microanalytical technique combining mass spectrometry and gas chromatography for the qualitative as well as quantitative determinations of compounds. Chromatography, Gas-Liquid-Mass Spectrometry,Chromatography, Gas-Mass Spectrometry,GCMS,Spectrometry, Mass-Gas Chromatography,Spectrum Analysis, Mass-Gas Chromatography,Gas-Liquid Chromatography-Mass Spectrometry,Mass Spectrometry-Gas Chromatography,Chromatography, Gas Liquid Mass Spectrometry,Chromatography, Gas Mass Spectrometry,Chromatography, Mass Spectrometry-Gas,Chromatography-Mass Spectrometry, Gas,Chromatography-Mass Spectrometry, Gas-Liquid,Gas Chromatography Mass Spectrometry,Gas Liquid Chromatography Mass Spectrometry,Mass Spectrometry Gas Chromatography,Spectrometries, Mass-Gas Chromatography,Spectrometry, Gas Chromatography-Mass,Spectrometry, Gas-Liquid Chromatography-Mass,Spectrometry, Mass Gas Chromatography,Spectrometry-Gas Chromatography, Mass,Spectrum Analysis, Mass Gas Chromatography
D010063 Ovum A mature haploid female germ cell extruded from the OVARY at OVULATION. Egg,Egg, Unfertilized,Ova,Eggs, Unfertilized,Unfertilized Egg,Unfertilized Eggs
D012015 Reference Standards A basis of value established for the measure of quantity, weight, extent or quality, e.g. weight standards, standard solutions, methods, techniques, and procedures used in diagnosis and therapy. Standard Preparations,Standards, Reference,Preparations, Standard,Standardization,Standards,Preparation, Standard,Reference Standard,Standard Preparation,Standard, Reference
D002853 Chromatography, Liquid Chromatographic techniques in which the mobile phase is a liquid. Liquid Chromatography
D013058 Mass Spectrometry An analytical method used in determining the identity of a chemical based on its mass using mass analyzers/mass spectrometers. Mass Spectroscopy,Spectrometry, Mass,Spectroscopy, Mass,Spectrum Analysis, Mass,Analysis, Mass Spectrum,Mass Spectrum Analysis,Analyses, Mass Spectrum,Mass Spectrum Analyses,Spectrum Analyses, Mass
D013449 Sulfonamides A group of compounds that contain the structure SO2NH2. Sulfonamide,Sulfonamide Mixture,Sulfonamide Mixtures,Mixture, Sulfonamide,Mixtures, Sulfonamide

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